CN103756787A - Method for extracting essential oil from wood processing waste Chinese fir chips to co-produce chemical method activated carbon - Google Patents
Method for extracting essential oil from wood processing waste Chinese fir chips to co-produce chemical method activated carbon Download PDFInfo
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Abstract
The invention proposes a method for extracting essential oil from wood processing waste Chinese fir chips to co-produce chemical method activated carbon. The method comprises the following steps: distilling fresh Chinese fir chips by water vapor; carrying out oil-water separation on condensate to obtain fir essential oil after cooling by obtained vapor; mixing the Chinese fir chips with a phosphoric acid according to the mass ratio of pure phosphoric acid to absolute dry sawdust of (1.8-3.0):1 after extracting oil; adding a cocatalyst concentrated sulfuric acid to fully mix according to the ratio of 1-8% of mass of the phosphoric acid, and then feeding to a sealed insulating barrel to carry out low-temperature osmotic treatment at 30-90 DEG C for 1-48 hours; carrying out carbonization, activation and post-treatment on the chemical method activated carbon; or carrying out plastifying, kneading, molding, drying and solidifying, carbon activation and post-treatment to obtain the chemical method granular activated carbon. Wooden column activated carbon can be prepared under the condition of not adding a binder, so that a plurality of purposes of efficient and comprehensive utilization of wastes, reduction of natural resource exploitation, reduction of environmental pollution, energy conservation and emission reduction are achieved.
Description
Technical field
The invention belongs to chemical technology field, is that a kind of wood working waste cedar sawdust extracts essential oil coproduction active carbon by chemical method technology.
Background technology
China fir is the important commerical tree species of China, wide at south China distributed pole, the wherein west and south, Hunan, and Jiangxi, Southern Zhejiang and Guangdong, Guangxi and the north, Fujian are the producing regions, center of China fir.According to the 4th national continuous forest inventory, add up: China Fir artificial forest area reaches 9,110,000 hm
2, account for 30.4% of national timber plantation area, total accumulation 3.4 hundred million m
3, the accumulation of many ripewoods can reach 105m
3/ hm
2, in national economy, occupy critical role.Jiangxi is one of the main distributed areas of China Fir and place of production, standing forest area approximately 140 ten thousand hms of the whole province take China fir as dominant tree
2, accounting for 30% of the whole province's forest total area, its growing stock is about fifty-five million m
3.Timber is produced after logging operation, will produce the lignocellulose wastes such as a large amount of cedar sawdusts, and cedar sawdust is a kind of raw material of good production gac, and since China starts to carry out Activated Carbon Production, cedar sawdust is all directly as raw material.And in fact in China fir, contain fir essential oil, be that one has high value-added product.
Essential oil (essential oil) be present in a class in plant materials can be with steam distillation, and there is the general name of the volatility oily liquid of certain fragrance.Fir essential oil is a kind ofly from China fir, to extract, colourless or micro-yellow, the transparent liquid with aromatising flavour.It has the strong banksia rose, Moschus, grane ambra fragrance, and the applicable illusion type essence of joining, is mainly used in makeup and soap class.In fir essential oil, cedar wood oil alcohol content is 60% left and right, and all the other also have α-pinene, chamene, pull fragrant alkene, alpha-terpineol, β-caryophyllene etc.Cedar wood oil alcohol is commonly called as cypress camphor, and existing market price is at 120 yuan of kg
-1left and right.Fir essential oil and China fir alkene are produced checking through throwing in, and can partly substitute cedar(wood)oil product completely.Duo Jia manufacturer is used at home, and has portioned product outlet, than using cedar(wood)oil to reduce costs more than 20%.Have good selling market, economic benefit is higher, aboundresources, and domestic every annual requirement reaches more than 1000 tons.Price 1.2 ten thousand～30,000 yuan per ton.
Fir essential oil is not only a kind of natural resource of preciousness, and the various compositions in fir essential oil also have pharmaceutical use.Chang ST finds in to fir essential oil termite-proof activity experiment, cedar wood oil alcohol has stronger termite-proof ability than α-cadinol, ferruginol, other terpenoid compositions in fir essential oil, have determined that to have the composition of physiologically active as follows: cypress camphor can play spasmolysis effect; α-pinene has obvious antibechic and the function of eliminating the phlegm, and has antimycotic (as Candida albicans) effect; Beta-pinene also has anti-inflammatory, dissolving phlegm, antifungic action; α-caryophyllene has antiasthmatic effect; Baras camphor resists myocardial ischemia, and promotes neurogliocyte growth, pain relieving, anticorrosion, anti-inflammatory etc.
The utilization of exploitation China fir resource in extraction of essential oil industry, both can alleviate China's natural plant essential oils demand and constantly increase the pressure bringing, and part replaces the widely cedar(wood)oil of application, can promote again China's forest zone expanding economy.
Cedar sawdust is through the pre-treatment of certain technique, extract fir essential oil, its residuum goes the charcoal processing of moulding making machine again, and the more former wood chip moulding product of its outward appearance and intensity quality all declines to some extent, the economic worth producing is lower, causes the profit of China fir extraction essential oil industry not high.
In the processes such as the accumulating of the exploitation of industrial solvent production, Chemicals production, oil and processing, organic materials and family room, all can there is the generation of volatile organic matter (VOCs).And the kind of VOCs is many, substantially belong to toxic gas, the health of harm humans; Participate in forming photo-chemical smog and aerosol, contaminate environment; Halogenated hydrocarbon organism can damage the ozone layer.The pollution problem of VOCs has caused showing great attention to of the world, developed country just starts to have carried out strict VOCs emission standard many years ago, as the China of developing country, overriding concern is the pollution problem that solves VOCs at present, for the recovery of VOCs, pays close attention to few.China is every year because of the lightweight oil approximately 4.7 × 10 of vaporization losses
5t, can reduce the loss approximately 4.35 × 10 if carry out oil gas recovery
5t, its value is roughly equal to Renminbi 2 × 10
9unit.As can be seen here, if can reclaim cost-effectively the VOCs of VOCs, particularly high density, high value, what will bring is environmental protection, economy and healthy triple benefits, for the development and the social sustainable development that promote China's recycling economy, is also of far-reaching significance.In future, the recovery of VOCs will worldwide more and more be paid attention to.
Active carbon adsorption is that one of effective means of VOCs is reclaimed in current absorption, is applied to already the recycling of VOCs.The granular carbon with high-specific surface area and flourishing hole can, by VOCs molecular retention, reach the object of waste gas being carried out to isolation of purified.Germany Bayer company adopts D47/4 gac transformation acetone mixed gas, and the rate of recovery reaches more than 95%.Japan Bell company employing gac pressure-variable adsorption partition method is recovered to purity and reaches 98% alcohol product, and what the recovering of vaporized hydrocarbons of the U.S. adopted substantially is the gac of high butane working capacity.
Nowadays, the mankind's quality of life constantly promotes, city has substantially all been moved out of in the chemical plant of high pollution, like this, automobile just becomes urban air first pollution source to the pollution of environment, and automobile is mainly derived from the evaporation of vehicle exhaust and fuel oil-gas to the pollution of atmosphere, wherein tail gas pollution accounts for 70%, and fuel evaporation thing pollutes and accounts for 30%.The U.S. just studied and on automobile, uses charcoal absorption gasoline vapor as far back as the end of the sixties in last century, and because this activated carbon technology content is higher, market value is higher, and this special-purpose activated charcoal is domestic whole dependence on import at present, and import price is at 8～100,000 yuan/ton.Cui Guogen has applied for the patent of cedar sawdust prepared product logos gac after extracting fir essential oil, application number: 201010218281.X in July, 2010.This method product yield is low, and the cedar sawdust of 10-13 ton left and right could be produced 1 ton of gac, and wood chip consumption is larger, and the industrialization of the Physical wood dust shaped activated carbon of current activated carbon industry is not perfect, and production cost is higher, and the market competitiveness is not high; The high temperature that needs 1000 ℃ of left and right in production, energy consumption is higher, does not reach and fully utilizes the most efficiently cedar sawdust.
Summary of the invention
In order to solve the problem of prior art existence, the invention provides a kind of method of wood working waste cedar sawdust extraction essential oil coproduction active carbon by chemical method, there is China fir comprehensive utilization ratio high, the feature of gac quality better.
Wood working waste cedar sawdust extracts a method for essential oil coproduction active carbon by chemical method, with water vapor, fresh cedar sawdust is distilled, and the cooling rear phlegma of gained steam obtains fir essential oil after oily water separation; To carry after oil cedar sawdust and phosphoric acid, according to pure phosphoric acid and over dry wood chip mass ratio, mix as the ratio of 1.8～3.0:1, and after adding the promotor vitriol oil fully to mix according to 1%～8% ratio of phosphoric acid quality, then send into and at 30～90 ℃ of airtight insulated tanks, carry out low temperature osmotic and process 1～48h; By charing, activation and aftertreatment, obtain chemical method powdered carbon; Or by obtaining chemical method granulated active carbon after plasticizing, kneading, moulding, dry solidification, charcoal activation and aftertreatment.
During distillation, vapor temperature is 110 ℃, and distillation time is 3-4 hour, and the mass ratio of water and over dry wood chip is 7-8:1.
The concentration of phosphoric acid is 40%wt～70%wt.
Carry the cedar sawdust after oil, cross 10～60 mesh sieves and re-use.
The carbonization temperature of chemical method powdered carbon is 210～300 ℃, and carbonization time is 30～120 minutes, and activation temperature is 350～500 ℃, and soak time is 30～120 minutes.
100～150 ℃ of the plasticization temperatures of chemical method granulated active carbon, fusion time 60～120 minutes.
Mediate and adopt kneader to process 5-10 minute.
Adopt the moulding of hydraulic molding machine direct pressing.
Dry solidification temperature is 210～300 ℃, and the dry solidification time is 30～120 minutes.
Charcoal activation temperature is 350～500 ℃, and charcoal soak time is 30～120 minutes.
Beneficial effect
The present invention proposes cedar sawdust and extract fir essential oil coproduction multiple types activated carbon technology, reached high-efficiency comprehensive utilization waste, reduce natural resources exploitation, alleviated the multipurpose of environmental pollution and energy-saving and emission-reduction.The pore structure that the present invention also can be adsorbed according to different application, decolouring field is required is carried out directional preparation.
By extracting essential oil and its extraction essential oil residuum, prepare the combination of two techniques of active carbon by chemical method, realized the high-efficiency comprehensive utilization of discarded cedar sawdust, reduce environmental pollution, economize on resources, reduce production costs, increase economic efficiency, promote industrial competitiveness, for China's coordinated development of the economy and society provides support, meet the requirement of the relevant program for the development of science and technology of forestry.
Cedar sawdust extracts essential oil technique and being combined into one of Activated Carbon Production technology, carry the rear wood chip of oil and through chemical activation method, can prepare powdery and the granular carbon of high added value, and extracting in fir essential oil process because partial organic substances is extracted, make the intermolecular hole of cedar sawdust obtain more exposure, while being conducive to follow-up activation, the infiltration of activator to cedar sawdust, makes the more excellent gac of performance
And, the present invention proposes cryogenic seal tank immersion method, the object of this method is in heat-processed, can not cause the phosphoric acid concentration of wood chip dipping to change because of the evaporation of water vapor in order to guarantee, phosphoric acid molecules is penetrated in wood chip weave construction fully, avoided open type dipping constantly to raise along with the evaporation of water vapor causes phosphoric acid concentration, degree of steeping is not thorough, and does not penetrate into the in-house phosphoric acid of wood chip very easily because carrying secretly of water vapor evaporation caused the waste of phosphoric acid and the pollution of environment.By closed dipping method, can increase substantially the absorption property of gac.And in confined conditions low temperature osmotic process after when preparing granulated active carbon, need not add in addition tackiness agent can direct plastication, kneaded and formed.
Accompanying drawing explanation
Fig. 1 cedar sawdust extracts essential oil coproduction active carbon by chemical method techniqueflow chart.
Embodiment
The invention discloses a kind of wood working waste cedar sawdust and extract essential oil coproduction active carbon by chemical method technology, key step is as described below:
1) water vapor that adopts waste heat boiler to produce distills fresh wood chip, and vapor temperature is 110 ℃, and with the mass ratio 7-8:1 distillation 3-4 hour of water and over dry wood chip, mixing steam enters refrigerating work procedure, and phlegma obtains fir essential oil after oily water separation.
2) adopt in step 1) and carry the cedar sawdust after oil, according to phosphorus wood, than (pure phosphoric acid and over dry wood chip mass ratio) 1.8:1～3.0:1, quantitatively take phosphoric acid (40%～70%wt) and catalyzer, catalyzer add-on is 1%～8% of phosphoric acid liquid quality.After fully mixing, send in insulated tank and at 30～90 ℃, permeate 1～48 hour.The phosphoric acid of employing 40%～70% is more conducive to recycle.
3) produce powdered carbon: by step 2) in compound at 210～300 ℃, process 30～120 minutes.
4) then send into activation converter, at 350～500 ℃, activation treatment 30～120 minutes, obtains powdered carbon through aftertreatment.
5) produce granulated active carbon: by step 2) in compound plastics processing 60～120 minutes at 100～150 ℃.
6) will have in plastic material converter kneader and mediate 5～10 minutes, material proceeds to molding device after mediating evenly, and it is the columnar material of 2mm or 4mm that direct pressing becomes diameter, does not need to add in addition tackiness agent.
7) columnar material is proceeded to charing converter by conveying belt, at 210～300 ℃, retain 30～120 minutes, make the abundant dry solidification of material.
8) wait to solidify end, material is proceeded in activation converter, at 350～500 ℃, keep 30～120 minutes, after activation finishes, product is obtained after aftertreatment to finished product.
Embodiment 1:
1) the fresh cedar sawdust through screening that is 30% with pre-thermogenetic steam in waste heat boiler recovered carbon production process to water content distills, distillation temperature is 110 ℃, distill after 3 hours, effective constituent contained in cedar sawdust together enters refrigerating work procedure with steam, obtain liquid crude oil water, after oily water separation, obtain fir essential oil, residuum is for carrying the rear cedar sawdust of oil;
2) will carry the rear cedar sawdust of oil mixes than 2.0:1 according to phosphorus wood with 60%wt phosphoric acid liquid, and add the catalyzer vitriol oil (98%wt) according to 1% of phosphoric acid quality, compound is sent in sealed thermal insulating bucket at 70 ℃ constant temperature and is kept proceeding to charing converter after 3 hours and carry out charing, charring furnace temperature is 250 ℃, the residence time is 60 minutes, then send into activation converter, activation temperature is 450 ℃, soak time is 30 minutes, obtain activated material, again through reclaiming, rinsing, dry, the aftertreatments such as abrasive dust obtain powdered carbon, the performance of product: Methylene blue adsorption is 20ml/0.1g(285mg/g), iodine number is 1120mg/g, Caramel adsorption is 120%.
Embodiment 2:
1) the fresh cedar sawdust through screening that is 30% with the pre-thermogenetic steam in waste heat boiler recovered carbon production process to water content distills, distillation temperature is 110 ℃, distill after 3 hours, effective constituent contained in cedar sawdust together enters refrigerating work procedure with steam, obtain liquid crude oil water, after oily water separation, obtain fir essential oil, residuum is for carrying the rear cedar sawdust of oil;
2) will carry the rear cedar sawdust of oil mixes than 2.0:1 according to phosphorus wood with 65%wt phosphoric acid liquid, and add the catalyzer vitriol oil (98%) according to 2% of phosphoric acid quality, compound is sent in sealed thermal insulating bucket constant temperature at 80 ℃ and is kept proceeding to plasticizing converter after 1.5 hours, plasticization temperature is 150 ℃, the residence time is 1 hour, plasticizing material is sent into the column material that in oil press, forming diameter is 2mm after kneader is processed 10 minutes, then proceed to charing converter and carry out charing, charring furnace temperature is 280 ℃, the residence time is 70 minutes, then send into activation converter, activation temperature is 500 ℃, soak time is 30 minutes, obtain activated material, again through reclaiming, rinsing, the aftertreatments such as oven dry obtain granulated active carbon, the performance of product: Methylene blue adsorption is 17ml/0.1g (240mg/g), iodine number is 1156mg/g, butane working capacity is 12g/100ml, intensity is 91%, specific surface area can reach 2800m
2/ g.
Embodiment 3:
1) the fresh cedar sawdust through screening that is 30% with the pre-thermogenetic steam in waste heat boiler recovered carbon production process to water content distills, distillation temperature is 110 ℃, distill after 3 hours, effective constituent contained in cedar sawdust together enters refrigerating work procedure with steam, obtain liquid crude oil water, after oily water separation, obtain fir essential oil, residuum is for carrying the rear cedar sawdust of oil;
2) will carry the rear cedar sawdust of oil mixes than 2.0:1 according to phosphorus wood with 65%wt phosphoric acid liquid, and add the catalyzer vitriol oil (98%) according to 1% of phosphoric acid quality, compound is sent in sealed thermal insulating bucket at 70 ℃ constant temperature and is kept proceeding to after 2 hours plasticizing plasticizing converter plasticizing, plasticization temperature is 150 ℃, the residence time is 1 hour, plasticizing material is sent into the column material that in oil press, forming diameter is 4mm after kneader is processed 10 minutes, then proceed to charing converter and carry out charing, charring furnace temperature is 260 ℃, the residence time is 90 minutes, then send into activation converter, activation temperature is 500 ℃, soak time is 60 minutes, obtain activated material, again through reclaiming, rinsing, the aftertreatments such as oven dry obtain granulated active carbon, the performance of product: Methylene blue adsorption is 16ml/0.1g(225mg/g), iodine number is 1076mg/g, butane working capacity is 11g/100ml, intensity is 93%.
Claims (10)
1. wood working waste cedar sawdust extracts a method for essential oil coproduction active carbon by chemical method, with water vapor, fresh cedar sawdust is distilled, and the cooling rear phlegma of gained steam obtains fir essential oil after oily water separation; It is characterized in that, to carry after oil cedar sawdust and phosphoric acid, according to pure phosphoric acid and over dry wood chip mass ratio, mix as the ratio of 1.8～3.0:1, and after adding the promotor vitriol oil fully to mix according to 1%～8% ratio of phosphoric acid quality, then send into and at 30～90 ℃ of airtight insulated tanks, carry out low temperature osmotic and process 1～48h; By charing, activation and aftertreatment, obtain chemical method powdered carbon; Or by obtaining chemical method granulated active carbon after plasticizing, kneading, moulding, dry solidification, charcoal activation and aftertreatment.
2. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, during distillation, vapor temperature is 110 ℃, and distillation time is 3-4 hour, and the mass ratio of water and over dry wood chip is 7-8:1.
3. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, the concentration of phosphoric acid is 40%wt～70%wt.
4. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, carries the cedar sawdust after oil, crosses 10～60 mesh sieves and re-uses.
5. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, the carbonization temperature of chemical method powdered carbon is 210～300 ℃, carbonization time is 30～120 minutes, activation temperature is 350～500 ℃, and soak time is 30～120 minutes.
6. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that 100～150 ℃ of the plasticization temperatures of chemical method granulated active carbon, fusion time 60～120 minutes.
7. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, mediates and adopts kneader to process 5-10 minute.
8. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, adopts the moulding of hydraulic molding machine direct pressing.
9. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, dry solidification temperature is 210～300 ℃, and the dry solidification time is 30～120 minutes.
10. wood working waste cedar sawdust extracts the method for essential oil coproduction active carbon by chemical method according to claim 1, it is characterized in that, charcoal activation temperature is 350～500 ℃, and charcoal soak time is 30～120 minutes.
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